EP0738341B1 - Kollektor vorgesehen zum gebrauch beim enttinten von abfallpapier nach dem flotationsverfahren - Google Patents

Kollektor vorgesehen zum gebrauch beim enttinten von abfallpapier nach dem flotationsverfahren Download PDF

Info

Publication number
EP0738341B1
EP0738341B1 EP94919918A EP94919918A EP0738341B1 EP 0738341 B1 EP0738341 B1 EP 0738341B1 EP 94919918 A EP94919918 A EP 94919918A EP 94919918 A EP94919918 A EP 94919918A EP 0738341 B1 EP0738341 B1 EP 0738341B1
Authority
EP
European Patent Office
Prior art keywords
acid
collector
flotation
deinking
reaction
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP94919918A
Other languages
English (en)
French (fr)
Other versions
EP0738341A1 (de
Inventor
Peter Wallberg
Enn PÄÄRT
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bim Kemi AB
Original Assignee
Bim Kemi AB
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from SE9302174A external-priority patent/SE501465C2/sv
Application filed by Bim Kemi AB filed Critical Bim Kemi AB
Publication of EP0738341A1 publication Critical patent/EP0738341A1/de
Application granted granted Critical
Publication of EP0738341B1 publication Critical patent/EP0738341B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • D21C5/02—Working-up waste paper
    • D21C5/025—De-inking
    • D21C5/027—Chemicals therefor
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/64—Paper recycling

Definitions

  • the deinking can be divided in three different steps; 1) dissolution of recycled fibre and discharging printing-ink from the fibres, 2) dispersing printing-ink in the water phase and 3) separation of the printing-ink. These three steps are included in both flotation process and the washing process.
  • the method which one uses industrial depends on the requirements and conditions which are found where the activity is located.
  • the object of the flotation process concerning the deinking is to remove the very most amount of printing-ink from a recycled fibre suspension.
  • the first step is to solve the fibre and disengage the printing-ink. When this is accomplished the particles must be modified so that they obtain suitable physical and chemical characteristics so that they afterwards can be lifted to the surface and removed with help of air-bubbles.
  • Some parameters are important to be consider at the flotation, such as the size of the particle, airflow in the flotation cell, the size of the air-bubbles, temperature, flotation time, the concentration of the recycled fibres in the flotation cell, pH, the concentration of the chemicals as well as the degree of the hardness of the water.
  • the flotation process is carried out in such a manner that the recycled raw material of the fibre is poured out through mechanical treatment in combination with a concentration of the chemicals.
  • mechanical treatment Different methods concerning chemicals/the concentration of the chemicals and method to pour the raw material exist.
  • the purpose of the mechanical treatment is that the fibres should be rubbed against each other and that one in that way, together with the chemicals, should get an efficient discharging of print-ink.
  • a too strong mechanical influence causes great damages on the fibres and this is not desirable at the paper-making.
  • Sodium hydroxide is used to adjust pH to the alkaline level and to saponificate and/or hydrolyse the resin in the printing-ink.
  • the pH at, which the deinking occurs, 9.5 - 11.0 causes that the fibres swell and thereby become more flexible.
  • Adding NaOH to the mechanical pulps makes the pulp to turn yellow and become dark.
  • the concentration of NaOH must be optimized.
  • the alkalinity must be high enough, as mentioned earlier, to obtain good saponification and hydrolysis of resins, which are included in the printing-inks. A sufficient high pH also gives a good fibre flexibility as well as an optimal function of the hydrogen peroxide.
  • Hydrogen peroxide is used to discolour the chromophors, which are originate from alkaline pH in the pulp.
  • the perhydroxyl anion (HOO-) is the active bleach chemical.
  • the concentration of this is influenced by the following parameters: pH, temperature, dose of hydrogen peroxide and the concentration of the certain metal ions such as Fe, Mn, Cu and others.
  • the influence of the metal ions can be reduced by adding chelate and sodium silicate. Certain microorganisms can also have negative influence by producing peroxide degrading enzymes.
  • Sodium silicate or water-glass, is a flotation silicate, which consists of SiO 2 and Na 2 O in varying mole ratio.
  • Sodium metal silicate has a mole ratio (Na 2 O/SiO 2 ) of approximately one and is the one mainly being used within the deinking. This is due to the higher alkalinity of the silicates with the low mole ratio.
  • the Silicate component is a mixture of many complex polymer silicate anions. By forming colloids with heavy metal ions the sodium silicate prevents a degradation of the hydrogen peroxide. The silicate even prevents the loose printing-ink from reprecipitating on the fibres.
  • the silicate has also a buffering effect on pH. Up to a certain level the brightness of the pulp increases with added concentration of the sodium silicate. However, the concentration of the silicate should be kept as low as possible, since problems with the deinkings in the subsequent equipment have been noted.
  • the printing-ink from the office waste form thin flake at the deinking. These are to big to be able to be removed by flotation or washing and to little to be able to be removed through filtration. If a chemical that changes the surface structure of the platform is added, they can be made to form agglomerate, which can be removed, e.g. through centrifugation.
  • the group of surface-active substances include many subgroups. For instance dispersing substances, collectors, substances with wetting characteristics, substances that prevents redeposition and so on, can be mentioned.
  • the surface-active substances being used for deinking will have two important components. A portion of the molecule must be hydrophillic and the other one must be of hydrophobic quality.
  • the structure of the surface-active substances can be a straight chain, branched chain, they can have charged groups, long or short chain, double or simple bindings and so on.
  • DTPA diethylentriaminpentaacetic acid
  • EDTA ethylendiamintetraacetic acid
  • the complex builders act by building solvable complexes of heavy metal ions. The complex prevents these ions from breaking down the hydrogen peroxide.
  • DTPA which has a structure with five "legs” is a more efficient complex builder than EDTA, which has a structure with four "legs”.
  • the hydrophobic surface structure favours an adsorption to air-bubbles.
  • the adsorption can be explained using surface chemistry, whereby through an interface between the air and the water the hydrophobic matters are oriented against the air phase. This occurs because it is advantageous from an energy point of view.
  • a surface-active chemical To be able to achieve a hydrophobing of the particles, one can add a surface-active chemical.
  • the conventional type of flotation chemical has required a high degree of hardness of the water to obtain intended effect. This acquires problem with depositions in form of CaCO 3 in the equipment.
  • so-called synthetic collector which do not require a high water hardness.
  • SE-B-464 639 a synthetic collector, which consists of a polyester based on a polyalkyline glycol and a di or tricarboxylic acid is described.
  • Tall oil is used of the polymerization reaction to control the chain length of the resulting polymer.
  • the collector produced in this manner is efficient and also non-polluting, as it is biologically degradable.
  • enhancements for example the possibility of controlling the polymerization reaction and the chain length of the polyester.
  • the object of the invention is to obtain an efficient synthetic collector, where the polymerization reaction can be controlled in a better way to thereby increase the reproducibility and give a more well-defined product.
  • the environmental aspects applying the biological degradability should be satisfied.
  • polyester obtained through reaction between 1) poly alkyline glycol, 2) di- and/or tricarboxylic acid and/-or anhydrides thereof as well as 3) any of the following saturated fatty acids: stearic acid, myristic acid and/or lauric acid, and, which polyester shows a molecular weight between 3000 - 10000.
  • Fig. 1 is a block diagram showing the brightness increase at flotation experiment with a collector according to the invention by different dosages.
  • Fig. 2 is a block diagram showing the brightness increase at flotation experiment with a collector according to the invention and a commercial collector.
  • the collector is a polyester made of a pokalkyline glycol and a di and/or tricarboxylic acid or its anhydrides.
  • a pokalkyline glycol Preferably, as polyalkyline glycol polyethylene glycol, PEG, HO-(CH 2 -CH 2 O) n -H and/or polypropylene glycol, PPG, HO-(CH 2 -CH 2 -CH 2 O) n -H are used. These can occur in several different molecular weights. We have used PEG as average molecular weight 400.
  • di or tricarboxylic acid is used maleine acid, fumaric acid, adipine acid, citric acid, oxalic acid or sebacic acid or its anhydrides. Mixtures can also be used.
  • Tall oil consists of 25-30% resin acids and 70-75% fatty acids.
  • the portion of fatty acid in the tall oil is approximately 5% saturated, approximately 25% consists of oil acid and approximately 70% consists of linolenic acid.
  • the mixture of different fatty acids makes it difficult to decide the appearance of the collector, but if estimation is done one can establish that the half the tall oil consists of linolenic acid.
  • a polyester was formed by gradually polymerization between two bi or multifunctional monomers.
  • a bifunctional monomer is meant a molecule with two functional groups.
  • the reaction is also called condensation polymerization because the water is separated.
  • condensation polymers are formed through gradually intermolecular condensation of reactive groups. Condensation polymers can also be formed through additional polymerisation. Bifunctional monomers give linear polymers, while polyfunctional gives branched or cross linked polymers. To interrupt the reaction one usually uses a monofunctional acid, which is called blockage acid.
  • the prerequisite for gradually polymerization is following:
  • the included raw materials were poured in a flange flask, the heating was started and the catalyst added. Timekeeping was started when the catalyst was added. Nitrogen was conducted in the mixture to obtain a certain stirring as well as to prevent oxygen supply. To improve the stirring a magnetic agitator was used. Water suction was used since low pressure lowers both partial pressures of water vapour in the flask and the boiling point at the reaction mixture.
  • the synthesis was accomplished at 150, 175 and 200°C respectively to be able to study the impact of the synthesis temperature on the molecular weight.
  • a double sample is performed to control the reproducibility for the synthesis.
  • the amount of the given water was measured and this condensate was controlled by means of FTIR.
  • the synthesis product was characterized by means of FTIR (Fourier Transform Infrared Spectroscopy), acid ratio, viscosity and in a certain case even by means of NMR (Nuclear Magnetic Resonance), clouding point and PLC (High Pressure Liquid Chromatography).
  • the amount of the included reactant was calculated through following method:
  • the slurry was poured in the flotation cell, which was filled with 40°C water. 1 litre was taken out for production of the brightness sheet and control of the white water purity.
  • the flotation chemicals were added in form of 0.75 g collector - 0.5% dosage. At flotation with soap based collector 0.3 g - 0.2% dosage was added. Also, 1.78 g CaCl 2 was added to obtain 7°dH.
  • the flotation was accomplished in 30 min. After the flotation, 10 litres were tapped from the cell and the sample was taken for brightness sheet and the water phase.
  • Brightness sheet was made according to SCAN standard C11:75. 1 litre sample was taken out from the flotation cell and poured in mixer so that the fibres were separated from each other. The mixture diluted to 2 litre and pH adjusted to 4.0 - 5.5. 4 samples of 0.5 litres were sucked out in Büchner funnel with the diameter of 11 cm. The sheet was pressed or rolled and dried in room temperature. The brightness was decided subsequently.
  • collectors were manufactured. By the attempts carried out, it was reviled that a collector based on polyethylene glycol, maleine acid and stearic acid gave the best result.
  • the molecular weight for the collector has been determine to approximately 6500 through HPLC.
  • the clouding point was 57°C.
  • the composition of the products and average molecular weight was controlled by means of NMR, FTIR and HPLC.
  • the viscosity measurements point out that the molecular weight increases with the synthetic temperature. Possibly a certain cross linking at higher temperature. Small differences in acid ratio but great differences in viscosity between the collector made at different synthetic temperatures indicates this.
  • the clouding point of the collector should be in few degrees above the flotation temperature. We recommend that a number of different collectors are produced for optimal performance when the flotation temperature varies between different deinking plants.

Landscapes

  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Toxicology (AREA)
  • Paper (AREA)

Claims (6)

  1. Kollektor zum Entfärben von Altpapier nach dem Flotationsverfahren,
    dadurch gekennzeichnet,
    daß er einen Polyester enthält, der durch die Reaktion zwischen 1) Polyethylenglykol, 2) Di-und/oder Tricarbonsäure und/oder Anhydriden davon als auch 3) irgendeiner der folgenden gesättigten Fettsäuren: Stearinsäure, Myristinsäure und/oder Laurinsäure erhalten wurde, wobei der Polyester ein Molekulargewicht zwischen 3000 - 10000 besitzt.
  2. Kollektor gemäß Anspruch 1,
    dadurch gekennzeichnet,
    daß die enthaltenen Ausgangsmaterialien nur aliphatische Carbonsäuren und Alkohole umfassen.
  3. Kollektor gemäß Anspruch 2,
    dadurch gekennzeichnet,
    daß das Polyalkylenglykol Polyethylenglykol ist, Polypropylenglykol oder Mischungen davon.
  4. Kollektor gemäß einem der vorhergehenden Ansprüche,
    dadurch gekennzeichnet,
    daß die Di- und Tricarbonsäure bevorzugt aus der Gruppe, bestehend aus Maleinsäure, Fumarsäure, Adipinsäure, Zitronensäure, Oxalsäure und Sebazinsäure oder Anhydriden von diesen, ausgewählt ist.
  5. Kollektor gemäß einem der vorhergehenden Ansprüche,
    dadurch gekennzeichnet,
    daß er durch Reaktion zwischen Polyethylenglykol, Maleinsäure und Stearinsäure hergestellt wird.
  6. Verwendung eines durch die Reaktion zwischen 1) Polyethyienglykol, 2) Di- und/oder Tricarbonsäure und/oder Anhydriden davon als auch 3) irgendeiner der folgenden gesättigten Fettsäuren: Stearinsäure, Myristinsäure und/oder Laurinsäure erhaltenen Polyesters als Kollektor zum Entfärben von Altpapier nach dem Flotationsverfahren, wobei der Polyester ein Molekulargewicht zwischen 3000 - 10000 besitzt.
EP94919918A 1993-06-23 1994-06-06 Kollektor vorgesehen zum gebrauch beim enttinten von abfallpapier nach dem flotationsverfahren Expired - Lifetime EP0738341B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
SE9302174A SE501465C2 (sv) 1992-12-07 1993-06-23 Samlare avsedd att användas vid avsvärtning av returpapper enligt flotationsprocessen
SE9302174 1993-06-23
PCT/SE1994/000547 WO1995000699A1 (en) 1993-06-23 1994-06-06 Collector intended to be used in deinking of waste paper according to the flotation process

Publications (2)

Publication Number Publication Date
EP0738341A1 EP0738341A1 (de) 1996-10-23
EP0738341B1 true EP0738341B1 (de) 1998-02-11

Family

ID=20390393

Family Applications (1)

Application Number Title Priority Date Filing Date
EP94919918A Expired - Lifetime EP0738341B1 (de) 1993-06-23 1994-06-06 Kollektor vorgesehen zum gebrauch beim enttinten von abfallpapier nach dem flotationsverfahren

Country Status (8)

Country Link
US (1) US5736622A (de)
EP (1) EP0738341B1 (de)
AT (1) ATE163205T1 (de)
AU (1) AU7087194A (de)
CA (1) CA2166092A1 (de)
DE (1) DE69408545T2 (de)
FI (1) FI109035B (de)
WO (1) WO1995000699A1 (de)

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SE9600730D0 (sv) * 1996-02-27 1996-02-27 Bim Kemi Ab Metod vid massatillverkning
WO2000051708A1 (en) * 1999-03-01 2000-09-08 Vulcan Performance Chemicals Polyester water-based defoamer
DE10138029A1 (de) * 2001-08-08 2003-02-27 Stockhausen Chem Fab Gmbh Verwendung von Emulsionen beim Deinking
US7862685B2 (en) * 2006-01-09 2011-01-04 Kemira Chemicals, Inc. Method for deinking pulp using premixed hydrophobically modified calcium carbonate particles
US7897010B2 (en) * 2006-01-09 2011-03-01 Kemira Chemicals, Inc. Method for deinking pulp using premixed hydrophobically modified calcium carbonate particles
US8052837B2 (en) * 2006-06-12 2011-11-08 Thiele Kaolin Company Deinking of waste paper
US8815051B2 (en) 2006-06-12 2014-08-26 Thiele Kaolin Company Deinking of waste paper
US8431232B2 (en) * 2008-10-30 2013-04-30 Eastman Chemical Company Aromatic-aliphatic polyester hot melt adhesives for roll-applied labels
US8317973B2 (en) * 2009-11-11 2012-11-27 Kemira Chemical, Inc. Polyester surfactants for deinking
US11447914B2 (en) 2017-12-07 2022-09-20 Thiele Kaolin Company Removal of stickies in the recycling of paper and paperboard

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2441025C3 (de) * 1973-08-29 1978-10-26 Mitsubishi Rayon Co. Ltd., Tokio Schwundarm härtbare ungesättigte Polyesterharzgemische und deren Verwendung für Formkörper mit verbesserter Haftfähigkeit für Überzüge
US4010126A (en) * 1975-04-11 1977-03-01 Celanese Corporation Aqueous emulsion copolymers of vinyl alkanoates, alkyl, acrylates, and acrylic modified alkyds
SE464639B (sv) * 1989-08-30 1991-05-27 Bim Kemi Ab Samlare avsedd att anvaendas vid avsvaertning av returpapper baserad paa en polyester som innefattar bl a tallolja och anvaendning av denna polyester som samlare
DE3943112A1 (de) * 1989-12-27 1991-07-04 Henkel Kgaa Wasserverduennbare bindemittelgemische auf basis von alkydharzen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DIALOG INFORMATION SERVICES, File 351, Derwent WPI, Dialog Accession No. 003525055, WPI Accession No. 82-73041E/35, HONSHU PAPER MFG KK et al.: "Removing Ink from Waste Printed Paper in Flotation Process Using Cpd. Obtd. by Addn. Polymerising Alkylene Oxide with Mono or Polyfunctional Alcohol and Reacting the Prod. with Dicarboxylic Acid; Polyester Pulp"; & JP,A,57117690, A, 820722, 8235 (BASIC) *

Also Published As

Publication number Publication date
ATE163205T1 (de) 1998-02-15
US5736622A (en) 1998-04-07
WO1995000699A1 (en) 1995-01-05
AU7087194A (en) 1995-01-17
FI956223A (fi) 1996-01-30
CA2166092A1 (en) 1995-01-05
DE69408545D1 (de) 1998-03-19
FI956223A0 (fi) 1995-12-22
FI109035B (fi) 2002-05-15
EP0738341A1 (de) 1996-10-23
DE69408545T2 (de) 1998-10-01

Similar Documents

Publication Publication Date Title
EP0738341B1 (de) Kollektor vorgesehen zum gebrauch beim enttinten von abfallpapier nach dem flotationsverfahren
US4147681A (en) Stable, self-inverting water-in-oil emulsions
US4077930A (en) Self-inverting emulsions of dialkyldiallyl ammonium chloride polymers and copolymers
Miao et al. Advances in the Control of Dissolved and Colloidal Substances Present in Papermaking Processes: A Brief Review.
JP2008502812A (ja) 古紙の脱インキ方法
WO1993017177A1 (en) Wastepaper deinking process
EP0060104B1 (de) Trocknung von Holzpulpe
US5266166A (en) Methods for controlling the deposition of organic contaminants in pulp and papermaking processes using a polyalkylene oxide/vinyl acetate graft copolymer
US5415733A (en) Method of removing hydrophilic ink
EP0737774B1 (de) Verfahren zur Behandlung des Abfalles aus einer Anlage zum Deinken von Altpapier
CN102391713B (zh) 含有木素改性产物的脱墨剂及其制备方法
AU2011215742A1 (en) Method for removing ink from paper
CN102532980A (zh) 一种中性生物酶脱墨剂及其制备方法
CA2112771C (en) Composition for producing paper and process for using same
US5501769A (en) Pulping wood using fatty acid esters of polyoxyalkalene glycols to enhance pulping uniformity and pulp yield
JP2001507408A (ja) 古紙からのインクの除去方法
CN103881468A (zh) 一种环保型混合废纸脱墨剂的制备原料及方法
WO1991003599A1 (en) Collector chemical for deinking of waste paper
US5658427A (en) Ethoxylated soya glycerides with glycols as deinking collector modifiers
Svensson The influence of surfactant chemistry on flotation deinking
AU695974B2 (en) Waste paper treatment process
EP0885326A1 (de) Chemikalien und verfahren zum deinken von altpapier
CN109280417A (zh) 中性脱墨剂及其制备方法
SE501465C2 (sv) Samlare avsedd att användas vid avsvärtning av returpapper enligt flotationsprocessen
CN109989292A (zh) 一种淀粉基固着剂的制备方法

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 19960117

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE DE FR GB NL SE

17Q First examination report despatched

Effective date: 19961202

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAG Despatch of communication of intention to grant

Free format text: ORIGINAL CODE: EPIDOS AGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAH Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOS IGRA

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE DE FR GB NL SE

REF Corresponds to:

Ref document number: 163205

Country of ref document: AT

Date of ref document: 19980215

Kind code of ref document: T

REF Corresponds to:

Ref document number: 69408545

Country of ref document: DE

Date of ref document: 19980319

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 19980511

ET Fr: translation filed
PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

26N No opposition filed
REG Reference to a national code

Ref country code: GB

Ref legal event code: IF02

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: GB

Payment date: 20020515

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: FR

Payment date: 20020625

Year of fee payment: 9

Ref country code: BE

Payment date: 20020625

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: NL

Payment date: 20020627

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: AT

Payment date: 20020630

Year of fee payment: 9

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20021129

Year of fee payment: 9

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030606

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030606

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20030630

BERE Be: lapsed

Owner name: *BIM KEMI A.B.

Effective date: 20030630

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040101

Ref country code: DE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040101

GBPC Gb: european patent ceased through non-payment of renewal fee

Effective date: 20030606

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: FR

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20040227

NLV4 Nl: lapsed or anulled due to non-payment of the annual fee

Effective date: 20040101

REG Reference to a national code

Ref country code: FR

Ref legal event code: ST